CN104677771B - A method of shale porosity is determined based on magnetic suspension gravimetric method - Google Patents

A method of shale porosity is determined based on magnetic suspension gravimetric method Download PDF

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CN104677771B
CN104677771B CN201510137730.0A CN201510137730A CN104677771B CN 104677771 B CN104677771 B CN 104677771B CN 201510137730 A CN201510137730 A CN 201510137730A CN 104677771 B CN104677771 B CN 104677771B
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sample
gas
volume
quality
porosity
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CN201510137730.0A
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CN104677771A (en
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王兴建
刘启鑫
田同辉
徐耀东
晁静
孟祥豪
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成都理工大学
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Abstract

The present invention provides a kind of methods for determining shale porosity based on magnetic suspension gravimetric method, method includes the following steps: carrying out quality and volume that skip test obtains sample;Carry out buoyancy test and calculate sample and sample bucket quality sum and volume and;Carry out the quality that absorption test obtains the gas of sample absorption;After reaching equilibrium state, the fact that the quality and constancy of volume of adsorbed gas, the porosity of sample is calculated according to the above-mentioned data of acquisition.The beneficial effects of the present invention are: the present invention utilizes gravimetric method isothermal adsorption principle, indirect measuring goes out the porosity of shale on the basis of accurately measuring the adsorbance of shale samples, has not only saved cost, also improves efficiency.

Description

A method of shale porosity is determined based on magnetic suspension gravimetric method

Technical field

The present invention relates to the technical fields of mineral measurement, more particularly to one kind to determine shale based on magnetic suspension gravimetric method The method of porosity.

Background technique

In order to measure the quality and pore abundance of reservoir rock porosity, and characterize the big of total pore volume in rock It is small, propose the concept of rock porosity (or porosity).Reservoir rock porosity may be defined as the total volume Vp of blowhole with The ratio between the total volume of rock Vr indicates, generally percentage that expression formula is as shown in 1-1-1 with Greek alphabet Φ:

Φ=Vp/Vr*100%=Vp/ (Vs+Vp) (1-1-1)

In formula, Φ-porosity, %;

Vr-rock sample total volume, cm3

Vp-pore volume, cm3

Vs-rock sample skeleton volume, cm3

When determining porosity, the total volume of rock, the volume of solid portion (particle and cement) and hole are only required to obtain Two among these three parameters of gap volume can calculate porosity by formula 1-1-1.

The measurement of sample solid volume mainly has bottle method, solid hydrometer method, submergence weight method, gas compression method. First three measuring method highlights gas since the restriction by pore size and experimental precision is less common here Compression method.With gas compression method method manufacture instrument, principle be all based on boyle-mariotte's law, it is right The sample of big rock core and small rock core, irregular figure and irregular contour is applicable.Instrument mainly has gas source, pressure regulator valve, high-precision Spend pressure gauge, sample room and normal volume room composition.Gas pours normal volume room V1 first, and records pressure P1.Then cut It dies source, the indoor gas of normal volume is put into sample room and makes up to pressure balance, thus can calculate rock solid Volume.Its calculating is as follows:

The volume of setting sample room is known as V2, when being wherein placed with the rock sample that one piece of solid volume is Vm, if gas Body is in Isothermal Condition, and pressure changes to P2 by P1, then has:

V1P1=V1P2+ (V2-Vm) P2

Then:

VmP2=V1P2+V2P2-V1P1

The solid volume of sample is are as follows:

Vm=V2+V1 (1-P1/P2) (1-1-2)

The measurement of rock sample pore volume

The measurement of rock sample pore volume mainly has saturation flow process and gas expansion method.The fluid one that saturation flow process uses As be kerosene or salt water, due to the influence of fluid polarity and surface tension of liquid, within the scope of rock sample compression strength, fluid without Method enters in shale nanoscale hole.In order to which more accurately measurement rock sample hole, general selection gas molecule make probe, because This, highlights the method for gas expansion method measurement rock sample pore volume here.Traditional gas expansion method is using a water Air pumping in rock sample is separated out, and measures the amount of the air by silver-colored volume pump, as the pore volume of the sample.Measurement institute The instrument used is Boyle's law porosimeter,

Sample is placed in the sample room of mercury volume pump, is that the mercury face at bend pipe both ends is equal, in the feelings that valve is opened Under condition, the pipe by mercury volume pump in left side is increased, and makes mercury face be more than sample, and reach at valve.The work of this process With being that other all air in sample room and pipe will be discharged in addition to the air in rock sample.At this point it is possible to directly read The total volume Vt of sample.Close valve, the mercury face on the left of bend pipe is reduced to sample room once, at this time the gas in sample by Vacuum is caused in sample room and is isolated.Again by the mercury face horizontalization of mercury volume pump two sides, at this time in valve sky below Between be exactly the amount of air isolated from sample.

According to boyle-mariotte's law, have

Vp Δ H=VHatm (1-1-3)

In formula, volume of air in Vp-hole, cm3

The volume that V-is precipitated from sample, cm3

Vacuum degree caused by Δ H- mercury pump, mmHg column;

Mercury under Hatm-atmospheric pressure, mmHg column.

Then porosity:

Vp=VHatm/ Δ H (1-1-4)

Currently, mainly using gas (generally He) as measurement intermediary.According to Boyle-Marriote's law, in perseverance Determine at temperature, core chamber's given volume, solid phase (particle) volume for being put into core chamber's sample is smaller, then body shared by core chamber's gas Product is bigger, and after being connected to standard chamber, balance pressure is lower;Conversely, balance bigger when being put into the indoor rock sample solid volume of rock core Pressure is higher.

Disadvantage of the prior art is that gas expansion method using gas as measurement intermediary, will receive the coefficient of viscosity and Immerse the influence of volumetric errors.In this experiment adjust reset pressure be not easy to adjust, when close to reset pressure value be easy by The determination of pressure value is influenced to the ownness of operator.The weight that adsorbance and porosity are evaluated and developed as shale reservoir Parameter is wanted, the prior art needs different laboratory apparatus to complete the measurement of the two, increases a large amount of financial resources cost and time Cost, and precision is not high.

Summary of the invention

The purpose of the invention is to overcome the deficiencies of the prior art and provide one kind to determine page based on magnetic suspension gravimetric method The method of petrosal foramen porosity.

The present invention is realized by above technical scheme:

The present invention provides a kind of method for determining shale porosity based on magnetic suspension gravimetric method, this method includes following step It is rapid:

Carry out quality and volume that skip test obtains sample bucket;

Carry out buoyancy test and calculate sample and sample bucket quality sum and volume and;

Carry out the quality that absorption test obtains the gas of sample absorption;

According to the quality and volume of the sample of acquisition, the quality sum of sample and sample bucket and volume and and sample absorption The Mass Calculation of gas obtain the porosity of sample.

Preferably, the quality and volume for carrying out skip test and obtaining sample bucket specifically:

Select N2As experimental gas.By booster pump by gas pressurized into measuring chamber, measure and record different pressures Under, the reading of magnetic suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate is established Rectangular coordinate system, and straight line is fitted according to the experiment value of acquisition, and calculate the quality and volume of sample bucket.

It is preferred it is described carry out buoyancy test and calculate sample and sample bucket quality sum and volume and specifically:

Select He as experimental gas.By booster pump by gas pressurized into measuring chamber, measure and record different pressures Under, the reading of magnetic suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate is established Rectangular coordinate system, and lines are fitted according to the experiment value of acquisition, and calculate the quality sum and volume of sample and sample bucket With.

Preferably, the quality for carrying out absorption test and obtaining the gas of sample absorption specifically: selection CH4As experiment Gas.By booster pump by gas pressurized into measuring chamber, measure and record under different pressures, the reading of magnetic suspension balance.It surveys After amount, using gas density as abscissa, magnetic suspension balance reading establishes rectangular coordinate system for ordinate, and according to acquisition Experiment value fits lines, obtains the quality of the gas of sample absorption.

It further include preferably volume correction, specifically, with formula mbal=(msc+ms+ma)-ρ·(vsc+vs+va) in density p For abscissa, mbalFor ordinate mapping, when sample reaches adsorption equilibrium, above-mentioned formula becomes using ρ as abscissa, mbalFor The linear function of ordinate, the 1-3 pressure spot mapping after taking experiment to reach balance, the slope of the straight line is vs、vsc、vaThree The sum of person;And according to Φ=va/(vs+va) * 100% calculate sample porosity, wherein mbalFor the balance matter in skip test Amount reading, mscFor sample bucket quality, msFor sample quality, vscFor sample bucket volume, vsFor sample volume, ρ is to test in absorption In gas density;Φ is porosity.

The beneficial effects of the present invention are: shale gas is mainly present in shale with absorption and free state, absorption therein contains The 20-80% between reserves is measured, therefore, the precise measurement of gas absorption amount and porosity is shale gas evaluating reservoir and exploitation Basis.Traditional adsorbance and porosity measurement need two different laboratory apparatus, and the at high cost and time is slower, and precision is not It is high.The present invention utilizes gravimetric method isothermal adsorption principle, and indirect measuring goes out on the basis of accurately measuring the adsorbance of shale samples The porosity of shale, has not only saved cost, also improves precision and efficiency.

Detailed description of the invention

Fig. 1 is the quality and density relationship figure in the embodiment of the present invention in skip test;

Fig. 2 is the balance schematic diagram in the embodiment of the present invention in buoyancy test;

Fig. 3 is measured value schematic diagram during the absorption in the embodiment of the present invention is tested;

Fig. 4 is the relational graph of density and quality in the embodiment of the present invention;

Fig. 5 is the relational graph of density and quality in the embodiment of the present invention.

Specific embodiment

In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.

The embodiment of the invention provides a kind of method for determining shale porosity based on magnetic suspension gravimetric method, this method includes Following steps:

Carry out quality and volume that skip test obtains sample bucket;

Carry out buoyancy test and calculate sample and sample bucket quality sum and volume and;

The quality of carry out product and the quality sum and volume of volume, sample and sample bucket and and sample absorption gas Mass Calculation obtains the porosity of sample.

It is therein, the quality and volume for carrying out skip test and obtaining sample bucket specifically:

Select N2As experimental gas.By booster pump by gas pressurized into measuring chamber, measure and record different pressures Under, the reading of magnetic suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate is established Rectangular coordinate system, and straight line is fitted according to the experiment value of acquisition, and calculate the quality and volume of sample bucket.

It is therein it is described carry out buoyancy test and calculate sample and sample bucket quality sum and volume and specifically:

Select He as experimental gas.By booster pump by gas pressurized into measuring chamber, measure and record different pressures Under, the reading of magnetic suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate is established Rectangular coordinate system, and lines are fitted according to the experiment value of acquisition, and calculate the quality sum and volume of sample and sample bucket With.

It is therein, the quality for carrying out absorption test and obtaining the gas of sample absorption specifically: select CH4 as experiment Gas.By booster pump by gas pressurized into measuring chamber, measure and record under different pressures, the reading of magnetic suspension balance.It surveys After amount, using gas density as abscissa, magnetic suspension balance reading establishes rectangular coordinate system for ordinate, and according to acquisition Experiment value fits lines, obtains the quality of the gas of sample absorption.

Therein further includes volume correction, specifically, with formula mbal=(msc+ms+ma)-ρ·(vsc+vs+va) in density p For abscissa, mbalFor ordinate mapping, when sample reaches adsorption equilibrium, above-mentioned formula becomes using ρ as abscissa, mbalFor The linear function of ordinate, the 1-3 pressure spot mapping after taking experiment to reach balance, the slope of the straight line is vs、vsc、vaThree The sum of person;And according to Φ=va/(vs+va) * 100% calculate sample porosity, wherein mbalFor the balance matter in skip test Amount reading, mscFor sample bucket quality, msFor sample quality, vscFor sample bucket volume, vsFor sample volume, ρ is to test in absorption In gas density;Φ is porosity.

It can be seen from the above description that shale gas is mainly present in shale with absorption and free state, absorption therein Content is between the 20-80% of reserves, and therefore, the precise measurement of gas absorption amount and porosity is shale gas evaluating reservoir and opens The basis of hair.Traditional adsorbance and porosity measurement need two different laboratory apparatus, and the at high cost and time is slower, this hair Bright to utilize gravimetric method isothermal adsorption principle, indirect measuring goes out the hole of shale on the basis of accurately measuring the adsorbance of shale samples Porosity has not only saved cost, also improves precision and efficiency.

Understanding to the present embodiment for convenience, is below described in detail it with specific step.

Experiment is divided into 3 steps: skip test, buoyancy test, absorption test.The purpose of skip test is to calculate sample bucket Quality mscWith volume vsc, using Archimedes buoyancy equilibrium principle, obtain such as formula 2-2-1:

Fbalanced=mscG-F floats (2-2-1)

Formula both sides are obtained divided by gravitational constant g simultaneously:

mbalanced=msc-ρ*vsc (2-2-2)

In formula, mbalanceBalance quality readings, g;

mscSample bucket quality, g;

vscSample bucket volume, cm3

Buoyancy test purpose is to calculate sample and sample bucket quality sum msc+msWith the sum of volume vsc+vs, utilize Archimedes buoyancy equilibrium principle is obtained such as formula 2-2-3:

Fbalanced=(msc+ms) g-F float (2-2-3)

Formula both sides are obtained divided by gravitational constant g simultaneously:

mbalanced=(msc+ms)―ρ*(vsc+vs) (2-2-4)

In formula, mbalanced- balance quality readings, g;

msc- sample bucket quality, g;

ms- sample quality, g;

vsc- sample bucket volume, cm3

vs- sample volume, cm3

Absorption test purpose is the quality m in order to calculate adsorbed gasa, using Archimedes buoyancy equilibrium principle, obtain To formula 2-2-5:

Fbalanced=(msc+ms+ma) g-F float (2-2-5)

It divided by gravitational constant g and transplants simultaneously on formula both sides:

ma=mbalanced+ρ*(vsc+vs+va)-(msc+ms) (2-2-6)

In formula, msc- sample bucket quality, g;

ms- sample quality, g;

ma- gas absorption amount, g;

vsc- sample bucket volume, cm3

vs- sample volume, cm3

va- adsorbed gas volume, cm3

Specific steps are as follows:

1. skip test selects N2As experimental gas.By booster pump by gas pressurized into measuring chamber, measure and remember It records under different pressures, the reading of magnetic suspension balance.After measurement, using gas density as abscissa, magnetic suspension balance reading is Ordinate establishes rectangular coordinate system, as shown in Figure 1.

2. buoyancy is tested, select He as experimental gas.By booster pump by gas pressurized into measuring chamber, measure and remember It records under different pressures, the reading of magnetic suspension balance.After measurement, using gas density as abscissa, magnetic suspension balance reading is Ordinate establishes rectangular coordinate system, as shown in Figure 2:

3. absorption test, selects CH4As experimental gas.By booster pump by gas pressurized into measuring chamber, measurement simultaneously It records under different pressures, the reading of magnetic suspension balance.After measurement, using gas density as abscissa, magnetic suspension balance reading Rectangular coordinate system is established for ordinate, as graphically shown in fig. 3:

4. formula 2-2-6 is deformed into following form by volume correction:

mbal=(msc+ms+ma)-ρ(vsc+vs+va) (2-2-7)

It is abscissa, m by density p in formula 2-2-7balIt maps (as shown in Figure 4) for ordinate, the deformation formula is negligible maAnd vaThe influence generated is calculated formula, and Direct Variable only has ρ and mbal

The curve initial stage is ma、va、ρ、mbalIt is the unknown curve of variable, when sample reaches adsorption equilibrium, i.e. sample When the quality and constancy of volume of product adsorbed gas, 2-2-7 formula at this time becomes using ρ as abscissa, mbalIt is the one of ordinate The form of secondary function y=kx+b takes experiment to reach 1-3 pressure spot after balance, again fitting mapping (such as Fig. 5).

The slope of straight line is vs、vsc、vaThe sum of three, the known v in blank and buoyancy experiments、vsc, V can be solveda

5. porosity calculation

Φ=va/(vs+va) * 100% (2-2-8)

2.3 technical solution of the present invention bring beneficial effects

Shale gas mainly with absorption and free state be present in shale, it is therein absorption content between reserves 20-80%, Therefore, gas absorption amount and the precise measurement of porosity are the bases of shale gas evaluating reservoir and exploitation.Traditional adsorbance Two different laboratory apparatus are needed with porosity measurement, the at high cost and time is slower, and the present invention utilizes gravimetric method isothermal adsorption Principle, indirect measuring goes out the porosity of shale on the basis of accurately measuring the adsorbance of shale samples, has not only saved cost, Also improve precision and efficiency.

The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.

Claims (1)

1. a kind of method for determining shale porosity based on magnetic suspension gravimetric method, which comprises the following steps:
Quality and volume that skip test obtains sample bucket are carried out, specifically:
Select N2As experimental gas, by booster pump by gas pressurized into measuring chamber, measure and record under different pressures, magnetic The reading of suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate establishes right angle seat Mark system, and linear fit is carried out according to the experiment value of acquisition, and calculate the quality and volume of sample bucket;
Carry out buoyancy test and calculate sample and sample bucket quality sum and volume and, specifically:
Select He as experimental gas, by booster pump by gas pressurized into measuring chamber, measure and record under different pressures, magnetic The reading of suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate establishes right angle seat Mark system, and according to the experiment value of acquisition carry out linear fit, and calculate sample and sample bucket quality sum and volume and;
The quality that absorption test obtains the gas of sample absorption is carried out, specifically:
Select CH4As experimental gas, by booster pump by gas pressurized into measuring chamber, measure and record under different pressures, magnetic The reading of suspension balance, after measurement, using gas density as abscissa, magnetic suspension balance reading is that ordinate establishes right angle seat Mark system, and linear fit is carried out according to the experiment value of acquisition, obtain the quality of sample adsorbed gas;
It further include volume correction, specifically, with formula mbal=(msc+ms+ma)-ρ·(vsc+vs+va) in density p be abscissa, mbalFor ordinate mapping, when sample reaches adsorption equilibrium, above-mentioned formula becomes using ρ as abscissa, mbalFor ordinate Linear function, the 1-3 pressure spot mapping after taking experiment to reach balance, the slope of the straight line is vs、vsc、vaThe sum of three; And according to Φ=va/(vs+va) * 100% calculate sample porosity, wherein mbalFor CH4It is adsorbed when as experimental gas Magnetic suspension balance reading when test, mscFor sample bucket quality, msFor sample quality, vscFor sample bucket volume, vsFor sample body Product, ρ are the gas density in absorption test;Φ is porosity;
According to the quality and volume of the sample bucket of acquisition, the quality sum of sample and sample bucket and volume and and sample absorption The Mass Calculation of gas obtains the porosity of sample.
CN201510137730.0A 2015-03-26 2015-03-26 A method of shale porosity is determined based on magnetic suspension gravimetric method CN104677771B (en)

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CN105181558B (en) * 2015-11-02 2017-09-26 太原理工大学 The test device and method of testing of deposit porosity
CN105445159A (en) * 2015-11-11 2016-03-30 成都理工大学 Method for obtaining pore diameter distribution curve and sample specific surface area
CN106198297B (en) * 2016-06-24 2019-08-02 西南石油大学 A method of accurately calculating methane true adsorbance on shale
CN107870136B (en) * 2016-09-28 2020-02-21 中石化石油工程技术服务有限公司 Method for measuring cationic degree of zwitterionic sulfonated phenolic resin
CN107271314A (en) * 2017-05-24 2017-10-20 中国矿业大学 A kind of method for measuring coal petrography adsorption swelling coefficient
CN108593497A (en) * 2018-05-30 2018-09-28 中国工程物理研究院激光聚变研究中心 A kind of accurate method for measuring self-supporting beryllium film density
CN108982328B (en) * 2018-08-14 2019-09-27 中南大学 A kind of method that rock pore volume deforms under calculating unfreezing
CN109269938A (en) * 2018-09-26 2019-01-25 西安石油大学 A kind of test method of coal and rock real density
CN110146409B (en) * 2019-05-09 2020-07-07 中国地质大学(武汉) Method for determining shale gas saturation based on density
CN110095375B (en) * 2019-05-14 2020-07-28 中国石油大学(北京) Shale gas content testing device and method

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